mickyfinn (Stranger)
06-10-03 04:16
No 439028
      Curbshot Nano Redeux...  Bookmark   

Well, they say that the third time is the charm...(whoever they is)

1G E
3G i2 crystals
125ml pyrex rb flask
small crock pot with sand inside

Ingredients went in according to the curbshot spec, the ballon was taped and the flask shaken well (with a finger covering the flask opening with the balloon.) Immediately, there is gas in the balloon, things bubbling madly in the flask which is then set in the sand inside the crock pot.

PROBLEM? The sand was not hot yet....will this ruin SWIM?

A towel is used to cover crock-pot replacing the lid since the top needs to accomodate the flask and balloon....but it doesn't seem to be bubbling like mad, if at all, as it was initially. It has been 10 minutes and the unit is now heating the flask....SWIM remembers post by O that visual indication is not necessary for a reaction to occur.

Is SWIM screwed, blued and tattood? SWIM gonna go kissin' a movin' train if this one fails....

Quick peak at small part of flask under towel reveals no perceptible activity. However, what can be observed of the fluid along the interior looks like candy apple red on a corvette.

Help SWIM Obie Wan Kenobi, you're SWIMFINN only hope....

Little Red Corvette...baby your much too fast...
(Stoni's sexual toy)
06-10-03 04:28
No 439031
      I hope you will enjoy your iodometh.  Bookmark   

I hope you will enjoy your iodometh.

I'm not fat just horizontally disproportionate.
06-10-03 04:47
No 439033
      Thanks for the semi-clue....  Bookmark   

I hope you will enjoy your iodometh.

SWIM glad Crotchety Obie Wan make fun of newbee SWIM... Bad Obie Wan...newbee clearly unmatched and easy target. WTF?

Got the drift and point (although wrapping the present in a wad of GAAK verbage leaves something to be desired.)

For anyone interested in helping newbee to dream first dream...the balloon swelled to double 1 hour into the reaction. SWIM pinched the balloon and slipped thumb over most of opening...then added 3-4 drops dh20 to the rxn and (OMG what the smell of that smoke is nASTy) re-attached the balloon without losing any (hardly any it seems) of the ballon contents and returned to crock pot sand bath.

SWIM wants to follow the post reaction workup by geezer and could use some indication from experienced bee as to whether this is a good idea and whether the addition of the 3-4 drops dh20 was enough...hope so as I'm off to sleep...but first...

Searched for iodometh and found present in snide comment...so a thank you to O is in order.


the priest said have mercy...let's burn him instead.
(Title Addict/Eraser)
06-10-03 06:01
No 439049
      ...  Bookmark   

they,  heh.  swij knows they.  but anyway...  jetson used to fuk with small nano's all the time(probably still does according to some bees standards,  under 10g=nano?)  and has found that small rxn to be inconsistant and therefore has scaled up a bit.  it's sometimes hard to tell if it went at all or is just burning away from the heat.  the only thing you can do now is to work it up and see what you end up with.  if your balloon swelled to double the size then swij would probably bet on conversion.  he's never had a balloon swell up past the initial standing up straight of one and has had some verry nice nano's.  just work it all up and keep your fingers crossed.  if you have decent lab techniques then you should end up with something.  at that small of a nano though one shouldn't put too much work into it.  may jetson suggest scaling up slightly?  it'll prove much easier to follow the rxn and easier to work up.  well good luck there mf.  oh and don't ge smelling the fumes and tell they to piss off....   they're always doing something to try and keep a bee down...

the devil is so lonelymad
(Stoni's sexual toy)
06-10-03 06:46
No 439061
      > 1G E > 2G MBRP > 3G i2 crystals...  Bookmark   

> 1G E
> 3G i2 crystals

Since you want the reaction to take place in strong, aqueous, about 55% HI I'd say you should have added about 1-1.5ml (=1-1.5g) of H2O at the beginning.
Since it is probably too late and that much water might quench the reaction since most of the I2 has already reacted I'd add about 0.5-0.75ml of water and hope for the best. Since you used quite a lot of I2 the conversion of the precursor and the final yield should be pretty good.

Next time you do such a reaction add the pfed + rP to the flask, followed by the water, and then add the I2 in 2-3 portions. No drama, no gas losses, a quiet reaction, and after a few hours reflux you're done.

I'm not fat just horizontally disproportionate.
06-10-03 13:16
No 439139
      Clear rxn fluid...  Bookmark   

Thanks again...

SWIM anxious to test the suggested volume of DH2O at the beginning next time and in a 3x larger dream, especailly since the pair of 200mm alihn condensors appeared finallly...not sure what r/p is recoverable/left yet so can't say when that 3G dream will begin. SWIM's looking forward to the Geezball Express® write up but not looking forward to makin more of that mbrp crap...plus need to research quantities until that write-up appears.

SWIM let the rxn just go for a few (4) hours at low low heat...woke up and there was precipitation of yellow droplets throughout the flask. Cooled to room temp and removed balloon. There was quite a bit of smoke and STENCH when opened (OMG that is nASTy.)

Warm DH2O swirled in rxn vessel, r/p drops free. Filtered through patented Charmin Plug®, and then passed through 30ml 30m Kimax buchner filter...volume of rxn fluid now 50-75ml...nearly clear like tap water. Not sure what constitutes from what the "original volume" would be comprised in regards to the suggestion that the rxn fluid be diluted to 3x original volume...guessing entire contents and volumetrically it's currently about 3x and situated in a 500ml rb flask awaiting n/p wash.

Off to figure out how to ghetto a separatory funnel till one appears on the local front as previous attempts at seperation leave MUCH to be desired. Don't want to jack this up by being "hasty" (gotta love those Ents.)

Trapped! -  Trapped in a world that...a world that he never made....
(Hive Bee)
06-10-03 14:43
No 439157
      before i got a sep funnel  Bookmark   

Before i got my sep funnel i would use one of those plastic syringes.  I would put a piece of 5mm id glass tubing on the end of it and use it to suck the bottom layer up while tilting the vessel.   A turkey baster should work as well but might be harder to control as you get the last bit.

It wasn't Me!
(Title Addict/Eraser)
06-10-03 15:49
No 439181
      ...  Bookmark   

jetson used to use a soda bottle(washed out well)  and a cap from a dish detergent bottle.

the devil is so lonelymad
06-10-03 23:52
No 439294
      blue base fluid?  Bookmark   

(side note) For some reason SWIM had to fall asleep for about 5 hours again and in the intervening time the clear rxn fluid became yellowish...the reason SWIM fell asleep was that he was waiting for last of DH20 wash of r/p in rxn vessel to filter through the aforementioned buchner filter)

50-75 ml rxn fluid was washed with xylene, tce and VM&P Naptha using one 200ml alihn condensor and fingertip for plug. Definitely ghetto and sucks...but better than a leaking device.

VM&P chosen as extraction vehicle and added to the rxn fluid which is still a bit light yellowish.

Decided to use baby bottle with nipple for ghetto sep funnel now...hope it works, thinkin it should.  SWIM intends to squeeze the nipple to adjust flow rate... cool

Following Geez post rxn workup the base solution was clear and warm, not room temp but close, and when poured into rxn fluid it was interesting to watch the process occur as written. Watching the base work SWIM forgot to smell along the way...then may have over based since the rxn solution was solid white and didn't do the 30 second clear. SWIM added warm DH20 and let it sit for 15 minutes. The base and rxn solution is blue and there is a thick layer of base solution at the bottom. Some fine solids are visible and not overpowering but discernable fish smell evident over the naptha.

<15 minutes later>

The rxn solution had cleard somewhat but still had a milky tint...decided to swirl and bring up to base. After letting it sit for 5 minutes SWIM went back in to smell...YECH!...SWIM guess we got amines cuz with a deep wif there was more pronounced fish rot smell. (hopefully this doesn't need to be on the scale of the rxn HI SUPERSTENCH which is just overpowering)

So....now SWIM will patiently let it sit for another 10 minutes and then proceed to the next phase which involves sacrifice and incantation SWIM believe....SWIM understand it's a bit like the body contortion involved in trying to get a UHF Television antenae to receive a signal. wink

Once again, thanks Os...SWIM'd certainly be sucking pond water right now if you hadn't pointed out SWIMFINN folly. SWIM may still end up bein' iodoboy but hopefully it will be less iodometh than it otherwise would have been .

you've got to break out, you got to proove you're alive...
(Hive Bee)
06-11-03 00:05
No 439296
      GhEtTo SePrAtOiEs  Bookmark   

A nice fairly precision ghetto sep funnel can bee had by taking any clear bottle that has a good seal to the cap, drill it, put a good rubber grommet in. (If you can find the right combo of cap/grommet, the OD of the grommet fits snugly inside the ID of the bottle top.) Now at the bottom of the bottle (the top when in use) a small 1/4" hole on the side (so it can still stand while being filled) this will require a little vinyl/rubber plug. FINALLY a snug fitting glass or plastic tube goes into the grommet, on the end of that tube, a couple inches of soft, clear vinyl hose.

TO USE: fill with any solutions that need sepping' put on the cap, and pinch the vinyl hose with hemostats.
Invert the bottle, and suspend with any reliable device that won't fail at the wrong time. Pull the little 1/4" plug and use the hemostats to regulate the flow from the bottle. The clear tube allows you to take the layer right to the "line".
Always replace the 1/4" plug once done with the flow. (BTW the 1/4" hole allows for a steady flow at the tube)
CODA: save up and buy a real sep funnel, and then MARVLE at the simplicity and ease of use. Be smart, and buy the shortest tip off the cock that is availible cos you are going to fucking break it ANYWAYS...

Once a dick always a dick. Once a bitch, well why do ya ask why he's a dick?
06-16-03 04:51
No 440283
      wet reflux  Bookmark   

SWIM took the goods from the new straight to e and daydreamed that approximately 1.5-2G psuedo - 1G MBRP (good quality) - approximately 2-3G i2 crystals and 2ml DH20 were combined in a 125ml pyrex rb flask (using Osmiums recommendation of 1ml Dh20 per 1G psuedo.) Added the items in the order recommended as well, shook the mix, attached standard balloon and then over that was taped a non-lubricated condom in case of leak or rupture. SWIM dreams he put it in crock pot sand bath for a few(going with 3 as a few)hours. If it should be a bit longer SWIM would love to know...

(no hillbilly trailers were filled with fireworks, smoke or harmed in any way as the result of this dream. This has been a public service announcement on behalf of hillbilly trailers everywhere...stop the madness!) wink

what makes you think that the weak survive?
(Of Counsel)
06-16-03 07:17
No 440293
      Let it go all day  Bookmark   

Leave it alone and let it go all day, 24 hours, 36 if you can stand it. At 1:1 with water and pseudo, my suggestion tends toward 36 hours.

Mostly harmless
06-16-03 12:32
No 440347
      additional time in reflux  Bookmark   

Leave it alone and let it go all day, 24 hours, 36 if you can stand it. At 1:1 with water and pseudo, my suggestion tends toward 36 hours.

hmmm, maybe SWIM doesn't love knowing that after all.winkJK! Thanks man!

SWIM's thingking it's got that unmistakable semi-sweet something smell down next to the flask...somehow the ballon did not get sealed well enough and has been seeping gas in very small quantities periodically. There it goes again...that smell...

<wander away from the keyboard...30 minutes later>

SWIM just realized this scent was referred to as "Rosebud" over 15 years ago in Northern California...it was noted for a particularly abrubt harsh sting when snorted, distinctive aroma and legs for days. SWIM hasn't had that pleasure in as many years...

<opps, wandered again...15 minutes later>

Well, SWIM pulled it off the sand since he failed to properly address the taping of the baloon this time and the aroma was getting a bit pungent for his liking and the plan was for three. It made most of about 8 hours it appears.

Tonight he wants to fire off two separate nano's with one each rp/i and H3PO3. The next rp/i will go to completion of 36 hours...the h3 probably 24 or so...still figuring.

Now, however it is time to kerplunk...

and once again kudos/thanks to VE for providing such absolutely reliable transportation to dreamland...always charging out at 105 C...

then have the guts to stand for somethin'or you're gonna be trapped!
06-16-03 17:43
No 440401
      Smelly balloon  Bookmark   

SWIM has found that even with the double balloon layer that the HI smell is still prevalent on the surface of the balloon. You're better off building a ghetto condensor from a fluoro light bulb (plans are in the SE and it's actually really simple), or even better get yourself the real deal. With a cooled condensor you can really just establish a proper reflux and leave it do its thing for however many hours you want without stressing about smells, balloons breaking etc.

With balloons SWIM also found that, especially with smaller flasks that were closer to the hot plate, the balloon didn't condense the excess gas properly and a lot of it stayed up in the balloon (although that probably could have been solved by cooking at a lower temperature).
(Hive Martyr)
06-16-03 18:09
No 440406
      Re: jetson used to use a soda bottle(washed...  Bookmark   

jetson used to use a soda bottle(washed out well)  and a cap from a dish detergent bottle.

I wonder if Jetson ever left his post-rxn lower layer in said soda bottle for say....a few days?

If so, I wonder what would happen to the integrity of said
soda bottle?

Has jetson ever had a 2 liter soda sep melt on him?

Swim has and would advise against using soda recepticals for sep funnels, unless! (big unless) one plans on using it for yanking out the goods and then transferring it into some other, more stable container.
Losing your 3rd and 4th pull due to laziness and ignorance isnt a fun experience. Especially when it's in the 1/2 to 3/4 oz range.

Buy a sep, skip the soda.

(Of Counsel)
06-17-03 07:50
No 440536
      soda bottles  Bookmark   

Ghetto sep funnel: three liter soda bottle with a quarter turn twist cap from a small Gatorade bottle (now available in two tone blue on Propel bottles). You can use this size bottle without a vent as it collapses sufficiently that no air is drawn back in through the cap when pouring out fluid.

The bottles stand up well enough to common solvents, but NaOH makes them brittle, and if you have the based reaction fluid in one, use it this time, and throw it away. You can buy generic soda in these bottles for as little as 89 cents in my area; the Gatorade costs more than that. I keep three or four around, even though I have a glass sep funnel. I have the hang of using them and the size is convenient for the way I tend to work. Never store based reaction fluid in a soda bottle, unless you just want to make a big mess.

Mostly harmless
06-17-03 16:43
No 440619
      *BUMP*  Bookmark   


I got lost now I'm so far behind...
(Title Addict/Eraser)
06-18-03 00:39
No 440736
      ...  Bookmark   

"I wonder if Jetson ever left his post-rxn lower layer in said soda bottle for say....a few days? "

well wonder no longer my friend.  believe it or not yes jetson has let it set for days.  and he means days.  with no problems with structural integrity of the bottle what so ever.  just the bottles in his area maybe?  perhaps.  perhaps he's just crazy and none of that really happened at all anyway...  who knows?  he sure doesn't anymore...

the devil is so lonelymad
(Hive Addict)
06-18-03 01:32
No 440754
      2 liter sep funnels  Bookmark   

These bottles work great! Swim has dreamed of leaving them (with caustic post rxn fluid) for up to two weeks.

The only problem is that eventually the plastic threads will corrode and become stripped. The cap will no longer bee air tight and will leak if turned upside down.

But if one chooses to use a turkey baster with a piece of plastic tubing for an extension and syphons his/her NP to canning jars for titration steps, after a couple of weeks most if not all of the theoretical gear should have fully migrated within this time frame anyway.
06-18-03 15:58
No 440903
      SWIM Day Afternoon  Bookmark   

That twist top from the Gatorade, of course! That is going to work nicely till the real thing...then medicine drop fine tuning removal of any overage.

Well, SWIM sucking pond water. Probably should have listened to geezer (ya think? To be fair though it was a smell issue with the baloon at that locale) but nooooooooooo. See the problem SWIM faces is that SWIM not sure what a rabbit looks like till SWIM sees the rabbit.


SWIM looks at rxn vessel and surmises that rxn has taken place based on SWIM best guess. So assuming for now that there was psuedo properly transformed SWIM decides to ker plunk and creates new nomencalture "ker-flunk, or how SWIM learned to suck pond water"

SWIM may have added a bit too much lye too quickly as almost immidiately (within 10 minutes) there was a rather white layer on the bottom half. There was also a very clearly identifiable mirror layer. Directly on the surface of the mirror there where bubbles surfacing, straining, bursting but not "like all get out". Shortly thereafter, there is a white substance that resembled honey wadding together directly on the surface of the mirror...eventually as SWIM was wondering at his new friend and adding little bits of lye and H202 his friend just withered away down below.

SWIM is freaking thinking he blew it, as now the surface is fading and pretty much nearly returnded to the original state it started - yellow. SWIM didn't have the ph tester and continued anyway hoping for the best.

There was no best to be found upon titrating...so SWIM went for the cabbage and now has a bottle for testing purposes. SWIM finds that both layers are about 8-9 today...is it possible to continue this dream?

In order to dream again SWIM's gotta run for supplies immediately since SWIM FUBAR'd the unFUBARable.

So be sure to join us next time sports fans when SWIM shows us how to FUBAR chewing bubble gum and walking

Sometimes I wonder, did you ever wonder what's become of little ol' me...
06-19-03 00:40
No 440972
      upgrading to glassware  Bookmark   

after a couple of weeks most if not all of the theoretical gear should have fully migrated within this time frame anyway.

That presupposes SWIM gets through an entire dream without having something go wrong. smile]end reply to the quote]

It also presupposes that other bees help SWIM with these obstacles even though he isn't a frickin' girl...

SWIM knows that other people are learning from SWIMS questions and obstacles so SWIM keeps going. Not completely for altruistic reasons but if SWIM can help a fellow bee he doesn't withold information or dole it out like some fuckin' miser....maybe people just don't read, SWIM doesn't know. SWIM's gonna get this though...you bet...

go ahead...ignore me.